Process of condensing glycerin.



W. RINTOUL da A. G. INNES. PROCESS 0F GONDENSING GLYGBRIN. APPLICATION FILED JUNE 17, 1911.

15.036,71 5 l Patented Aug. 27, 1912.

. m @LL/@g2g ff u.. 5y m insana To all whomt may concern:

Be it known that we, WILLIAM RINTOUL ICE.

WILLIAM EINTOUL AND ALFRED GEORGE INNES, F STEVENSTON, SCOTLAND, ASSIGN- ORS TO I. DU PONT DE NEMOURS POWDER COMANY, OF WILMINGTON, DELAWARE,

ACORPORATION OF'NEW JERSEY.

i i mi PROCESS 0F C'OND'N'SING GLYCERIN.

Sipeciieation' of Letters Patent. Patented Aug, 27, 1912'.

Application led .Tune 17, 1911. Serial No. 653,819.

` and ALFRED GEORGE NNES, subjectsvof the King of Great Britain, residing at Stevenston, Ayrshire, Scotland, have invented a" new and useful Improvement in l rocesses of Condensing Glycerin, of which the following is a full, clear, and exact description, reference being had 'to the apcompanying drawings, which form a part of this specification.

- Our invention relates to certain improvements -n the process for'the production of so-called condensed glycerin.

V By condensed glycerin is understood the condensation and simultaneous dehydration of som or all of the molecules of glycerin in groups of two, three or more,

- with formation of molecules of 'any or all of the following, viz: diglyoerin, triglycerin, tetraglycerin, and higher .products of condensation.

The present invention contemplates two distinct steps in the treatment of glycerinthe said steps being advantageously combined-of which the lirst has for its object f the avoidance of certain drawbacks attendto flow back through a-fcooling arrangement while the water vapor is allowed to escape. Now, under these conditions the drawback isv encountered that the condensation is acl," companied by'a partial decomposition of the glycerin. The condensed glycerin so formed is unsuitable 'for the manufacture from it of nitricI esters', inasmuch as the nitrated product is very diHicult to wash,

dry and stabilize, by reason of the readiness withpwhich' it forms slimy emulsions with water. It has also' been proposed to conduct theoperation of condensation' at a somewhat reduced temperaturer 1n a vacuum vessel.

yfrom whichntmospheric oxygen is excluded, `but even fthls` `alterr1at1ve methodis troubleratus. W e have discovered that this can be effected by heating the glycerin at ordinary pressures to temperatures lower than the boiling point. We have discovered that the action will proceed at all temperatures between 200 C. or even lower and 275 C., Without any of the drawbacks referred to.

At the lower temperatures at which we carry out the reaction larger 'quantitiesof soda, sodium acetate, etc., may be employed without rilsk of unduly decomposing the glycerin; whereby the reduction of the velocity of reaction due to the lower temperature is compensated for. ln order to accelerate this reaction by removing the water liberated as fast as it is formed, we bring in contact with the hot glycerin a stream or strea s of air or carbon dioXid or other suitable gas or vapor. 'At lower temperatures air can be employed without undue decomposition of the glycerin.. temperatures up to and including the boiling point, it is preferable to lemploy some' suitable gas or vapor having no oxidizing At h igher tendency/such for instance, as carbon dioXid. This, the second step of theprocess can be adopted with advantage, whether the glycerin be condensed at its boiling temperature, as in previous processes, or at temperatures below this, as in our improved process. f,

An apparat-us with which this-process may be carried out and which apparatus is claimed in a sepa-rate application, filed by us, `is illustrated in theaccompanying drawing in which a Vlsectional view of said apparatus is shown.

ons a metallic vessel preferably surrounded or covered with heat lnsulatmg material l). c is a steam coil in the interior of this' vessel.

,CZ is the steam inlet to the coil, and e the steam outlet. f is a pipe, having the stopcock g, for the admisison of the glycerin, to

vbe treated, into the interior of the vessel, and

h is the outlet pipe for the treated glycerin, said outlet pipe having the valve i. j is a gas inlet leading to the perforated ringsc at or, near the bottom of the vessel.

Z is a thermometer for determining the temperature.

' 0A is an exit through the cover offtheyesadmitted through the steam inlet at proper #the perforations in the rings la, The gas orl -as formed "by bringing a stream or streams v ing the glycerinto be condensed, and during ing Vthe vwater liberated as formed by. bring- 3.- The 'hereinbefore described- Iprocess of wings-the glycerin .to be condensed to a temperature lower than the boilinglpoint of the glycerin, and during said treatmentremoving ythe water liberated as formed by bringglycerin? -thiough said glycerin. n i The. hereinbefore described process of` sel'for the gases and vapors to escape, which exit may beconnected with a return cooler (not shown).

In practice the glycerin is admitted through the pipe f in measured quantities suiiicient to iil-l and maintain the liquid in the vessel a at a proper level, and steam is pressure and temperature to maintain the temperature inthe coil c at the proper temperature,` and gas orvapor is Aadmitted through the gas inlet and escapes through vapor after action on'the glycerin passes out of the apparatus through the pipe 0. The treated glycerin escapes through the pipe hl Having now described our invention what We claim and desire to secure Iby Letters Patent of the United States is (l, Thehereinbei'ore described process ofl condensing glycerin, which consists` in heating the. glycerin to be condensed to a temperaturev lower than the boiling point of the glycerin, `and duringsaid treatment removing astream or streams of a vapor in contact with said glycerin.

'2. The hereinbefore described process of condensing glycerin, which consists in heating the glycerin to be condensed, and during said treatment removing the waterI liberated of a-vaporf in'contact with said glycerin.'

condensingl glycerin, which consists in heating non-,oxidizing vaporinvcontact with said 4. The hereinbef'o're described process of condensing glycerin, which consists in heat' said treatment removing the water liberated as formed by forcing non-oxidizing vapor.v

condensing glycerin, which consistsin heating the glycerin to ble cond nsed to a teinperature lower than the boiling point of the glycerin, and during said treatment removing the water liberated as formed by forcing carbon-dioxid vapor through said glycerin.

6. The hereinbefore described process of condensing glycerin, which consists in heat-- ing the glycerin to be condensed, andduringv said treatment removing the water 'liberated as formed by forcing a stream or streams ot,V

a vapor through said glycerin.

9. The hereinbefore described process 1 of condensing glycerin, which consists in heating vthe glycerin to be condensed to a teinperature lower than the boiling pointl ofthe glycerin,l and during said treatment removing the water liberated as formed by forcing nonoxidizing vapor through said glycerin.

' j 10. `The hereinbefore described* process of condensing glycerin, which consists in heating the glycerin to be condensed, and during I said treatment removing the waterI liberated as formed by forcing non-oxidizingvapor '.th'rough ysaid glycerin.

'In testimony ofwhich invention, we have 23rd day of May,'191 1.

WILLIAM iuNToUL. l nALEEED GEORGE iNNEs.

i 'VVitnessesz- ,CnAvNsr'oN FAIRWEATHER,

Joiiri-MCCLnnRY.

"hereunto set-our hands, at Glasgowfon this Y 

